CN103225173A - Cellulose/carbon nano tube composite nanofiber membrane preparation method - Google Patents
Cellulose/carbon nano tube composite nanofiber membrane preparation method Download PDFInfo
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- CN103225173A CN103225173A CN2013101827337A CN201310182733A CN103225173A CN 103225173 A CN103225173 A CN 103225173A CN 2013101827337 A CN2013101827337 A CN 2013101827337A CN 201310182733 A CN201310182733 A CN 201310182733A CN 103225173 A CN103225173 A CN 103225173A
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Abstract
The invention discloses a cellulose/carbon nano tube composite nanofiber membrane preparation method, and belongs to an electroactive material preparation technology. The method comprises the following processes of: firstly, acidizing carbon nano tubes so as to enable CNT-COOH to be generated on the surfaces of the carbon nano tubes, and dispersing the carbon nano tubes into deionized water to prepare a carbon nano tube solution; dissolving bacterial cellulose into trifluoroacetic acid so as to obtain a transparent light-yellow bacterial cellulose trifluoroacetic acid solution; and mixing the carbon nano tube solution with the bacterial cellulose trifluoroacetic acid solution and electrospinning, wherein the high-voltage electrostatic regulation scope is 10-30kV, the flow rate of an injection pump is 0.05-0.3mL/h, and the receiving distance is 10-20cm. The preparation method is simple in process, and an obtained cellulose/carbon nano tube composite nanofiber membrane has the advantages of high electric conductivity and good electroactivity.
Description
Technical field
The present invention relates to a kind of cellulose/CNT (containing single wall and Duo Bi (n=2-20)) and carry out the preparation method of spinning film forming, belong to the technology of preparing of electroactive material by high-pressure electrostatic.
Background technology
Cellulose is the natural biological source macromolecular material the widest, that annual production is maximum that distributes on the earth, is real continuable, the natural material that can not consume.Cellulose has a lot of particular performances, as hydrophily, optical activity, biocompatibility etc.The most common, the most important source of cellulose mainly is cotton and timber, and in addition, fiber crops, straw, straw, bagasse etc. all are cellulosic abundant sources, and these are referred to as plant cellulose by the cellulose that plant obtains.1886Brown finds that first bacterium also can synthetic cellulose, and these are called bacteria cellulose by the cellulose that some bacterium of acetobacter, rhizobium, Agrobacterium, Sarcina etc. produces under certain condition.Wherein most representative bacterium is an acetobacter xylinum, and it is a kind of bar-shaped gram negative strain, and very suitable fermented-producing bacteria cellulose and the productive rate of being used for is bigger.Compare with plant cellulose, bacteria cellulose has some special advantages: purity height, mechanical performance that degree of crystallinity is big, excellent, good water retention property and hydrophily, have bioaffinity and biocompatibility.Its Application Areas is very extensive, mainly contains: medical material, food industry, paper industry, electronic equipment etc.Especially in recent years bacteria cellulose has caused people's attention in sensor research as electroactive material.
CNT is a kind of One-dimensional Quantum material with special construction, strengthens aspects such as body, semi-conducting material, catalyst carrier, nano composite material in the nanometer of engineering material and has wide potential using value.In addition, CNT has that good conjugated system, high electron affinity energy and energy of ionization, photostability are strong, excellent photoelectric performance and physical and mechanical properties make it have application prospects at aspects such as improving polymeric material optics, electricity, mechanics, calorifics.Along with the maturation of carbon nanotube preparation technology and the continuous reduction of CNT cost, the application study of CNT more and more becomes the emphasis of research.If it is compound that CNT and bacteria cellulose are carried out molecular level, carry out electrostatic spinning then, the electroactive material that then is expected to obtain having high electroactive performance.
Also do not relate at present the cellulose/preparation of CNT electroactive material and the report of aspect of performance and patent with high electroactive performance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of cellulose/CNT composite nano-fiber membrane makes material with this method and has high electroactive performance.
The present invention is realized by following technical proposals.The preparation method of a kind of cellulose/CNT composite nano-fiber membrane, this method is at first carried out acidification with CNT, make its surface have carboxyl (CNT-COOH), again it is carried out ultrasonic the mixing with bacteria cellulose in being dissolved in trifluoroacetic acid, by the composite nano-fiber membrane that the electrostatic spinning preparation has high electroactive performance, this method is characterized in that comprising following process:
1) carbon nano-tube solution preparation: single wall or multi-walled carbon nano-tubes are joined by quality HNO
3/ H
2SO
4Be in 1: 1 the mixed acid, be mixed with the solution of 0.01～0.1g/mL, solution is heated to backflow 60-90min under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is 5～15mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) cellulose solution preparation: at room temperature be that 20～600,000 bacteria cellulose is dissolved in the trifluoroacetic acid with molecular weight, be mixed with volume mass mark (g/L) and be 3～10% solution, magnetic agitation 6h obtains transparent light yellow cellulose trifluoroacetic acid solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the cellulose trifluoroacetic acid solution of acquisition was mixed according to the mass ratio of solute in 0.05: 1～0.25: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 10～30kV, syringe pump flow velocity 0.05～0.3mL/h, receiving range 10～20cm, obtaining directly is 60～150nm tunica fibrosa.
Preparation method's process of the present invention is simple, and the cellulose that obtains/CNT composite nano-fiber membrane has electrical conductivity height, advantage that electroactive performance is good.
The specific embodiment
Embodiment 1:
1) carbon nano-tube solution preparation: the HNO that the 4.0g Single Walled Carbon Nanotube is joined 200ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.02g/mL, solution is heated to backflow 60min under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 6.0mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) dimension cellulose solution preparation: at room temperature be that 500,000 bacteria cellulose is dissolved in the trifluoroacetic acid with certain molecular weight, be mixed with volume mass mark (g/L) and be 3.5% solution, magnetic agitation 6h obtains transparent light yellow cellulose trifluoroacetic acid solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the cellulose trifluoroacetic acid solution of acquisition is mixed according to the mass ratio of solute at 0.05: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 30kV, syringe pump flow velocity 0.05mL/h, receiving range 20cm, obtaining directly is 60～70nm tunica fibrosa.
Embodiment 2:
1) acidifying of nanotube: the HNO that the 4.0g Single Walled Carbon Nanotube is joined 100ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.04g/mL, solution is heated to backflow 70min under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 8.0mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) dimension cellulose solution preparation: at room temperature be that 400,000 bacteria cellulose is dissolved in the trifluoroacetic acid with certain molecular weight, be mixed with volume mass mark (g/L) and be 5% solution, magnetic agitation 6h obtains transparent light yellow cellulose trifluoroacetic acid solution;
3) composite solution preparation: the carbon nano-tube solution that step 1) is obtained, with carbon nano-tube solution and step 2) the cellulose trifluoroacetic acid solution of acquisition is mixed according to the mass ratio of solute at 0.1: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 25kV, syringe pump flow velocity 0.1mL/h, receiving range 15cm, obtaining directly is 80～100nm tunica fibrosa.
Embodiment 3:
1) acidifying of nanotube: the HNO that the 8.0g Single Walled Carbon Nanotube is joined 100ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.08g/mL, solution is heated to backflow 90min under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 10mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) dimension cellulose solution preparation: at room temperature be that 300,000 bacteria cellulose is dissolved in the trifluoroacetic acid with certain molecular weight, be mixed with volume mass mark (g/L) and be 7% solution, magnetic agitation 6h obtains transparent light yellow cellulose trifluoroacetic acid solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the cellulose trifluoroacetic acid solution of acquisition is mixed according to the mass ratio of solute at 0.15: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 20kV, syringe pump flow velocity 0.2mL/h, receiving range 20cm, obtaining directly is 100～120nm tunica fibrosa.
Embodiment 4:
1) acidifying of nanotube: the HNO that the 8.0g Single Walled Carbon Nanotube is joined 100ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.08g/mL, solution is heated to backflow 90min under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 12mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) dimension cellulose solution preparation: at room temperature be that 200,000 bacteria cellulose is dissolved in the trifluoroacetic acid with certain molecular weight, be mixed with volume mass mark (g/L) and be 9% solution, magnetic agitation 6h obtains transparent light yellow cellulose trifluoroacetic acid solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the cellulose trifluoroacetic acid solution of acquisition is mixed according to the mass ratio of solute at 0.20: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 30kV, syringe pump flow velocity 0.25mL/h, receiving range 15cm, obtaining directly is 120～150nm tunica fibrosa.
Claims (1)
1. the preparation method of cellulose/CNT composite nano-fiber membrane, this method is at first carried out acidification with CNT, make its surface have carboxyl (CNT-COOH), again it is carried out ultrasonic the mixing with bacteria cellulose in being dissolved in trifluoroacetic acid, by the composite nano-fiber membrane that the electrostatic spinning preparation has high electroactive performance, this method is characterized in that comprising following process:
1) carbon nano-tube solution preparation: single wall or multi-walled carbon nano-tubes are joined by quality HNO
3/ H
2SO
4Be in 1: 1 the mixed acid, be mixed with the solution of 0.01～0.1g/mL, solution is heated to backflow 60-90min under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is 5～15mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) cellulose solution preparation: at room temperature be that 20～600,000 bacteria cellulose is dissolved in the trifluoroacetic acid with molecular weight, be mixed with volume mass mark (g/L) and be 3～10% solution, magnetic agitation 6h obtains transparent light yellow cellulose trifluoroacetic acid solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the cellulose trifluoroacetic acid solution of acquisition was mixed according to the mass ratio of solute in 0.05: 1～0.25: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 10～30kV, syringe pump flow velocity 0.05～0.3mL/h, receiving range 10～20cm, obtaining directly is 60～150nm tunica fibrosa.
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Cited By (13)
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| CN104403131A (en) * | 2014-11-25 | 2015-03-11 | 苏州市贝克生物科技有限公司 | Carbon nano tube/bacterial cellulose medical composite film and preparation method thereof |
| CN104707171A (en) * | 2015-02-03 | 2015-06-17 | 天津大学 | Preparation method of bioactive glass nanotube |
| CN105111507A (en) * | 2015-09-08 | 2015-12-02 | 哈尔滨工业大学 | Preparation method and application of bacterial cellulose/polyaniline/carbon nanotube conducting film material |
| CN105977046A (en) * | 2016-07-28 | 2016-09-28 | 北京化工大学 | Integrated supercapacitor and manufacturing method thereof |
| CN106498625A (en) * | 2016-10-24 | 2017-03-15 | 天津工业大学 | A kind of poly butyric ester/carbon nano tube composite nanofiber membrane and preparation method thereof |
| CN106676946A (en) * | 2017-01-09 | 2017-05-17 | 云南中烟工业有限责任公司 | Multifunctional carbon nanotube composite packaging paper |
| CN106905562A (en) * | 2017-03-20 | 2017-06-30 | 江南大学 | A kind of bacteria cellulose in situ/functionalized multi-wall carbonnanotubes membrane material and preparation method thereof |
| CN108221465A (en) * | 2017-12-15 | 2018-06-29 | 复旦大学 | Cellulose nano-fibrous/fluorocarbons pipe flexible compound film and preparation method thereof |
| CN108532014A (en) * | 2018-04-10 | 2018-09-14 | 天津工业大学 | A kind of nanofiber electroactive polymer material and preparation method thereof |
| CN111826325A (en) * | 2020-08-05 | 2020-10-27 | 华创佳农生物科技(武汉)有限公司 | Application of multi-walled carbon nanotube in rhizobium inoculant and preparation method thereof |
| CN112216522A (en) * | 2019-07-12 | 2021-01-12 | 南京林业大学 | Electrostatic spinning flexible electrode material and preparation method thereof |
| CN114457622A (en) * | 2022-02-08 | 2022-05-10 | 丁国奥 | Moisture-proof and oxidation-resistant file box material and preparation method thereof |
| CN115341339A (en) * | 2022-08-25 | 2022-11-15 | 武汉大学 | Silk fibroin composite fiber membrane for detecting and analyzing perfluorinated polyfluoro compounds and method |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104403131A (en) * | 2014-11-25 | 2015-03-11 | 苏州市贝克生物科技有限公司 | Carbon nano tube/bacterial cellulose medical composite film and preparation method thereof |
| CN104707171A (en) * | 2015-02-03 | 2015-06-17 | 天津大学 | Preparation method of bioactive glass nanotube |
| CN105111507A (en) * | 2015-09-08 | 2015-12-02 | 哈尔滨工业大学 | Preparation method and application of bacterial cellulose/polyaniline/carbon nanotube conducting film material |
| CN105977046A (en) * | 2016-07-28 | 2016-09-28 | 北京化工大学 | Integrated supercapacitor and manufacturing method thereof |
| CN106498625A (en) * | 2016-10-24 | 2017-03-15 | 天津工业大学 | A kind of poly butyric ester/carbon nano tube composite nanofiber membrane and preparation method thereof |
| CN106498625B (en) * | 2016-10-24 | 2018-09-14 | 天津工业大学 | A kind of poly butyric ester/carbon nano tube composite nanofiber membrane and preparation method thereof |
| CN106676946A (en) * | 2017-01-09 | 2017-05-17 | 云南中烟工业有限责任公司 | Multifunctional carbon nanotube composite packaging paper |
| CN106905562A (en) * | 2017-03-20 | 2017-06-30 | 江南大学 | A kind of bacteria cellulose in situ/functionalized multi-wall carbonnanotubes membrane material and preparation method thereof |
| CN108221465B (en) * | 2017-12-15 | 2020-05-12 | 复旦大学 | Cellulose nano-fiber/carbon fluoride tube flexible composite membrane and preparation method thereof |
| CN108221465A (en) * | 2017-12-15 | 2018-06-29 | 复旦大学 | Cellulose nano-fibrous/fluorocarbons pipe flexible compound film and preparation method thereof |
| CN108532014A (en) * | 2018-04-10 | 2018-09-14 | 天津工业大学 | A kind of nanofiber electroactive polymer material and preparation method thereof |
| CN112216522A (en) * | 2019-07-12 | 2021-01-12 | 南京林业大学 | Electrostatic spinning flexible electrode material and preparation method thereof |
| CN111826325A (en) * | 2020-08-05 | 2020-10-27 | 华创佳农生物科技(武汉)有限公司 | Application of multi-walled carbon nanotube in rhizobium inoculant and preparation method thereof |
| CN114457622A (en) * | 2022-02-08 | 2022-05-10 | 丁国奥 | Moisture-proof and oxidation-resistant file box material and preparation method thereof |
| CN115341339A (en) * | 2022-08-25 | 2022-11-15 | 武汉大学 | Silk fibroin composite fiber membrane for detecting and analyzing perfluorinated polyfluoro compounds and method |
| CN115341339B (en) * | 2022-08-25 | 2024-03-22 | 武汉大学 | Silk fibroin composite fiber film and method for detecting and analyzing perfluoro-type compounds |
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